WO2016086529A1 - Composition d'organopolysiloxane thixotrope et dispositif à semi-conducteur - Google Patents

Composition d'organopolysiloxane thixotrope et dispositif à semi-conducteur Download PDF

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WO2016086529A1
WO2016086529A1 PCT/CN2015/072097 CN2015072097W WO2016086529A1 WO 2016086529 A1 WO2016086529 A1 WO 2016086529A1 CN 2015072097 W CN2015072097 W CN 2015072097W WO 2016086529 A1 WO2016086529 A1 WO 2016086529A1
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sio
thixotropic
component
composition according
weight
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PCT/CN2015/072097
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Chinese (zh)
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杨仕海
郑海庭
何海
朱经纬
黄光燕
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广州慧谷化学有限公司
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/4805—Shape
    • H01L2224/4809—Loop shape
    • H01L2224/48091—Arched
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/73—Means for bonding being of different types provided for in two or more of groups H01L2224/10, H01L2224/18, H01L2224/26, H01L2224/34, H01L2224/42, H01L2224/50, H01L2224/63, H01L2224/71
    • H01L2224/732—Location after the connecting process
    • H01L2224/73251—Location after the connecting process on different surfaces
    • H01L2224/73265—Layer and wire connectors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
    • H01L2924/181—Encapsulation

Definitions

  • the present invention relates to a silicone composition, and more particularly to a thixotropic organopolysiloxane composition, and a semiconductor device constructed using the composition cured.
  • the basic structural unit of the silicone polymer is composed of silicon oxide links, and the side chains are connected to various other organic groups through silicon atoms.
  • silicone polymers have the following outstanding properties: 1. Temperature resistance, silicone products are based on silicon-oxygen (Si-O) bonds, so the thermal stability of silicone products High, high temperature (or radiation) molecules do not break or break down chemical bonds. 2. Weather resistance, the main chain of silicone products is -Si-O-, which has better thermal stability than other polymer materials, and is resistant to radiation and weathering, and has a long service life in a natural environment. 3.
  • silicone products have good electrical insulation properties, dielectric loss, withstand voltage, corona resistance, volume resistivity and surface resistivity are among the best in insulating materials, and their electrical properties are affected by The effects of temperature and frequency are small. Therefore, based on the above-mentioned good comprehensive performance, as one of the silicone products, organopolysiloxane is widely used in the LED packaging and photovoltaic industries.
  • Patent Application Publication No. CN103342816A discloses a curable organopolysiloxane composition for use in an LED lamp package having the following advantages: excellent adhesion, strong hardness, and excellent resistance to thermal shock. High transparency.
  • an LED lamp package includes a light-emitting element and an LED holder, the light-emitting element is fixed on the LED holder, the LED holder is generally composed of a metal substrate, and a silver-plated layer is disposed on the metal substrate.
  • the silver plating layer is used for collecting or astigmatizing the light of the light-emitting element.
  • the organopolysiloxane composition is dispensed onto the silver-plated layer of the light-emitting element and the LED holder, and cured, that is, the packaging of the LED lamp is substantially completed.
  • the technical problem to be solved by the present invention is to overcome the above-mentioned drawbacks of the prior art and to provide a curable organopolysiloxane composition which is compatible with thixotropic properties and heat resistance and oil-reducing properties.
  • the present invention also provides a semiconductor device including a light-emitting element and a holder for fixing the light-emitting element, wherein the light-emitting element is coated with the thixotropic organic substance of the present invention A cured product of a silicone composition.
  • the thixotropic organopolysiloxane composition provided by the invention comprises:
  • (A1) a solid three-dimensional organopolysiloxane comprising R 1 3 SiO 1/2 units and SiO 4/2 units, R 1 being selected from the same or different alkenyl groups, containing no aromatic hydrocarbons and not containing aliphatic groups a monovalent substituted or unsubstituted hydrocarbon group of a saturated bond;
  • (A2) a liquid linear structure organopolysiloxane comprising R 1 3 SiO 1/2 units and R 2 2 SiO 2/2 units, and R 1 and R 2 are selected from the same or different alkenyl groups, and are not included a monovalent substituted or unsubstituted hydrocarbon group having an aromatic hydrocarbon and no aliphatic unsaturated bond, wherein the (A2) component has a number average molecular weight of less than 10,000;
  • (A3) a liquid linear structure organopolysiloxane comprising R 1 3 SiO 1/2 units and R 2 2 SiO 2/2 units, and R 1 and R 2 are selected from the same or different alkenyl groups, and are not included a monovalent substituted or unsubstituted hydrocarbon group having an aromatic hydrocarbon and not containing an aliphatic unsaturated bond, wherein the (A3) component has a number average molecular weight of more than 80,000;
  • component (A1) is a main component of the composition of the present invention, and alkenyl groups in components (A1) to (A3) are mutually reacted with silicon-bonded hydrogen atoms in component (B). Form a crosslink bond and cure.
  • the molecular structure of the component (A1) is a solid three-dimensional structure molecular chain structure, and should contain R 1 3 SiO 1/2 units and SiO 4/2 units in one molecule.
  • the alkenyl group in the component (A1) may be represented by a vinyl group, a propenyl group, a butenyl group, a pentenyl group and a hexenyl group, and most preferably a vinyl group.
  • the monovalent substituted or unsubstituted hydrocarbon group in the component (A1) which does not contain an aromatic hydrocarbon and does not contain an aliphatic unsaturated bond may include the following groups: methyl group, ethyl group, propyl group, butyl group, and pentyl group.
  • the alkenyl group is contained in an amount of from 0.01 to 0.30 mol / 100 g, preferably from 0.02 to 0.25 mol / 100 g.
  • the present invention has a number average molecular weight of preferably 2500-3500 in the component (A1), and when the number average molecular weight of (A1) is less than 2500, the initial adhesion force after curing is deteriorated; when (A1) When the number average molecular weight is more than 3,500, the hardness of the material after curing is too high, and the long-term work at high temperature is prone to cracking, causing the colloid to peel off from the substrate.
  • the (A1) has the following average unit molecular formula,
  • R 5 is selected from the same or different alkenyl groups
  • the alkenyl group in R 5 may be represented by a vinyl group, a propenyl group, a butenyl group, a pentenyl group and a hexenyl group, most preferably a vinyl group
  • a monovalent substituted or unsubstituted alkyl group is a methyl group, an ethyl group, or a propyl group.
  • the monovalent substituted or unsubstituted alkyl group in R 6 may include a group: methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl or the like, most preferably methyl.
  • the component (A1) may include the following formula as a representative:
  • component (A2) is one of the main components of the composition of the present invention, and the molecular structure of component (A2) is a liquid linear molecular chain structure, and should contain R 1 3 SiO 1/2 in one molecule. Unit and R 2 2 SiO 2/2 unit.
  • the alkenyl group reacts with the silicon-bonded hydrogen atom in the component (B) to form a cross-linking bond, and is cured.
  • the alkenyl group in the component (A2) may be represented by a vinyl group, a propenyl group, a butenyl group, a pentenyl group and a hexenyl group, and most preferably a vinyl group.
  • the monovalent substituted or unsubstituted hydrocarbon group in the component (A2) which does not contain an aromatic hydrocarbon and does not contain an aliphatic unsaturated bond may include the following groups: methyl group, ethyl group, propyl group, butyl group, pentyl group.
  • the content of the alkenyl group is preferably from 0.01 to 0.5 mol/100 g, preferably from 0.02 to 0.3 mol/100 g;
  • the number average molecular weight of the fraction (A2) is limited to less than 10,000, and when the number average molecular weight of (A2) is more than 10,000, there is a risk that the mold material is poor in moldability and the oil yield is increased during use.
  • the (A2) has the following average unit molecular formula,
  • R 5 is selected from the same or different alkenyl groups
  • R 6 is selected from the same or different monovalent substituted or unsubstituted alkyl groups, 1 ⁇ a3 ⁇ 130.
  • the alkenyl group in R 5 may be represented by a vinyl group, a propenyl group, a butenyl group, a pentenyl group and a hexenyl group, and most preferably a vinyl group.
  • the monovalent substituted or unsubstituted alkyl group in R 6 may include a group: methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl or the like, most preferably methyl.
  • the component (A2) may include the following molecular formula as a representative:
  • component (A3) is one of the main components of the composition of the present invention, and the molecular structure of component (A3) is a liquid linear molecular chain structure, and should contain R 1 3 SiO 1/2 in one molecule. Unit and R 2 2 SiO 2/2 unit.
  • the alkenyl group reacts with the silicon-bonded hydrogen atom in the component (B) to form a cross-linking bond, and is cured.
  • the alkenyl group in the component (A3) may be represented by a vinyl group, a propenyl group, a butenyl group, a pentenyl group and a hexenyl group, and most preferably a vinyl group.
  • the monovalent substituted or unsubstituted hydrocarbon group in the component (A3) which does not contain an aromatic hydrocarbon and does not contain an aliphatic unsaturated bond may include the following groups: methyl group, ethyl group, propyl group, butyl group, pentyl group.
  • the alkenyl group is contained in an amount of 0.0001 to 0.0025 mol/100 g, preferably 0.0002 to 0.002 mol/100 g;
  • the number average molecular weight of (A3) is limited to more than 80000, and when the number average molecular weight of (A3) is less than 80000, there is a risk that the rubber material may be inferior in flexibility and heat resistance may be lowered during use.
  • the present invention employs a linear structure (A2) having a number average molecular weight of less than 10,000 and a linear structure (A3) having a number average molecular weight of more than 80,000, the design makes the crosslink density of the low molecular weight structure large in the mixing process, and the reactivity is Strong and low-viscosity performance, while exerting the advantages of low cross-linking density and high heat-resistance of high-molecular-weight substances, the synergistic effect of the two, in the reaction of the rubber, the macromolecules and small molecules are entangled to form a staggered network structure.
  • the cross-linking density of the structure is between the two single materials, and the neutralization is affected by the poor heat resistance due to the high cross-linking density, and at the same time solves the serious influence of the oil due to the small cross-linking density; in addition, the cooperation of the two molecular weights
  • the function can neutralize the low viscosity of a single small molecule, resulting in insufficient molding height and poor flexibility. At the same time, it can solve the problem that the shape of the construction is not due to the high viscosity of a single macromolecule. Sleek effect.
  • the weight ratio between the components (A2) and (A3) is preferably from 99:1 to 1:99.
  • the ratio of the weight of the component (A1) to the sum of the weights of the components (A2) and (A3) ranges from 0.1:1 to 1.2:1.
  • the component (B) is one of the main components of the composition of the present invention, and the silicon-bonded hydrogen atom in this component reacts with the alkenyl group in the component (A1) and the component (A2). Form a crosslink bond and cure.
  • the molecular structure of the component (B) is a liquid linear molecular chain structure, and should contain R 3 3 SiO 1/2 units and R 4 2 SiO 2/2 units in one molecule.
  • the monovalent substituted or unsubstituted hydrocarbon group which does not contain an aromatic hydrocarbon and does not contain an aliphatic unsaturated bond in the component (B) may include the following groups: methyl group, ethyl group, propyl group, butyl group, pentyl group, hexyl group.
  • the silicon-bonded hydrogen atom content in the component (B) is from 0.1 to 1.5 mol/100 g, preferably from 0.2 to 1.5 mol/100 g.
  • the ratio of the silicon-bonded hydrogen atom in the component (B) to the molar amount of the alkenyl group in the components (A1) to (A3) is from 1.1 to 2.0.
  • the (B) has the following average unit molecular formula
  • the R 8 may include a group: methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl or the like alkyl, chloromethyl, 3-chloropropyl or similar alkyl halide The group is most preferably a methyl group.
  • the component (B) may include the following molecular formula as a representative:
  • the component (C) as a tackifier is one of the important components of the composition of the present invention, and this component organosiloxane has an average of at least one epoxy group in one molecule due to the component of the present invention ( The presence of an epoxy group in C) has a good adhesion to an iron substrate.
  • the epoxy equivalent is preferably from 150 to 500, and the molecular weight is preferably from 200 to 5,000.
  • the molecular structure of the component (C) is not particularly limited in the present invention, and may be an organosiloxane having a linear structure, a branched structure or a cyclic structure, and is preferably a linear or cyclic structure.
  • the (C) has the following molecular structural formula,
  • R is Or a hydrogen atom.
  • the component (D) is a thixotropic agent, also known as a anti-flowing agent, and its function is to enable the resin solution to have a high consistency at rest when it is added to the resin composition, and to become low under the action of an external force.
  • the principle is a large specific surface area material which can form a hydrogen bond with a polymer in a resin or some other structure, which can be thinned under stress and thickened upon standing.
  • the type of the thixotropic agent is not particularly limited, and various thixotropic agents in the art may be used, such as organic bentonite, hydrogenated castor oil or polyamide wax, LBCB-1 thixotropic lubricant, vinyl chloride compound, and hydrophobic gas phase. Silica and so on. Preferred is a thixotropic agent having a specific surface area of from 100 to 400 in an amount of from 3 to 30% by weight based on the total weight of the composition, and the present invention is preferably a hydrophobic fumed silica.
  • the component (E) is a catalyst which causes a hydrosilylation reaction between an alkenyl group in the components (A1) to (A3) and a silicon-bonded hydrogen atom in the component (B).
  • component (E) is a catalyst that promotes curing of the composition.
  • the type of the catalyst in the present invention is not particularly limited, and a catalyst conventionally used in the art may be, for example, a platinum catalyst, a rhodium catalyst or a palladium catalyst, and the present invention is preferably a platinum catalyst.
  • the present invention employs a platinum catalyst having tetramethylvinyldisiloxane as a ligand.
  • the amount of the component (E) to be used is not particularly limited, and it is preferably used in an amount sufficient to promote the curing reaction of the composition.
  • the curable organopolysiloxane composition of the present invention may further comprise a component (F) addition reaction inhibitor for the purpose of prolonging the shelf life of the curable organopolysiloxane composition of the present invention.
  • the addition reaction inhibitor is a temperature-dependent substance which rapidly loses its inhibition when heated to a certain extent, and causes the composition to undergo a curing reaction.
  • the kind weight and the addition amount of the addition reaction inhibitor of the component (F) are not particularly limited, and a conventional inhibitor in the art may be used, and the addition amount may be added as needed.
  • the component (F) in the present invention is an ethynyl ring. Hexanol is added in an amount of 0.01% by weight based on the total weight of the composition.
  • the preparation method of the components (A) to (F) is not particularly limited, and it can be obtained by a conventional method in the art, or is commercially available.
  • component (A1) is from 3 to 30% by weight based on the total weight of the composition; the sum of the components (A2) and (A3) by weight is from 40% by weight to 80% by weight based on the total weight of the composition; Component (B) is from 0.1% by weight to 30% by weight based on the total weight of the composition, and component (C) is from 0.01% by weight to 10% by weight based on the total weight of the composition.
  • the present invention also provides a process for preparing an organopolysiloxane composition by mixing components (A1) to (A3) with components (B), (C), (D) and (E), Further, the component (F) and other additives such as an inorganic filler, a pigment, a flame retardant, a heat resistant agent and the like are added as needed to prepare a curable organopolysiloxane composition.
  • a semiconductor device comprising a light-emitting element and a holder for fixing the light-emitting element, and the mixed composition is coated on a holder of the light-emitting element to be cured, for example, at 100 ° C After 1 h, and then cured at 150 ° C for 3 h, a cured body having a tensile strength greater than 1.0 MPa and an elongation at break greater than 80% at a temperature of 25 ° C and a humidity of 60% RH was formed.
  • the hardness values of the three points were measured using a Shore A hardness tester, and the hardness was greater than A30 and less than A60.
  • conventional organopolysiloxane compositions are difficult to form advantages with good heat and thixotropic properties.
  • composition of the present invention and the cured semiconductor device thereof not only maintain good heat resistance and oil-out performance, but also have good thixotropic properties.
  • FIG. 1 is a schematic cross-sectional view showing a package of a semiconductor device according to an embodiment of the present invention
  • LED holder 2. Light-emitting element; 3. Electrode; 4. Bonding line; 5. Cured body of curable organopolysiloxane composition.
  • Vi is a vinyl group
  • Me is a methyl group
  • MQ configuration means a three-dimensional structure having SiO 4/2 units
  • MD configuration means a linear structure having R 2 2 SiO 2/2 units.
  • An MQ configuration having a molecular weight of 3000 at 25 ° C, a phenyl group-free, and a vinyl compound having a vinyl molar content of 0.10 mol/100 g.
  • the MQ configuration having a molecular weight of 2,500 at 25 ° C, containing no phenyl group, and having a vinyl molar content of 0.11 mol/100 g of an organosilicon compound.
  • the MQ configuration having a molecular weight of 3,500 at 25 ° C, containing no phenyl group, and having a vinyl molar content of 0.09 moles per 100 g of the organosilicon compound.
  • the MD configuration at a molecular weight of 4,600 at 25 ° C, without a phenyl group, and a vinyl molar content of 0.04 moles per 100 g of organosilicon compound.
  • An MD configuration having a molecular weight of 300,000 at 25 ° C, a phenyl group free, and a vinyl compound having a molar content of 0.0006 moles per 100 g.
  • An MD configuration having a molecular weight of 20,000 at 25 ° C, a phenyl group free, and a vinyl molar content of 0.01 mol / 100 g of an organosilicon compound.
  • the phenyl group is not contained, and the hydrogen molar content is 0.5 mol / 100 g of the organosilicon compound, and the molecular formula is as follows:
  • An organosilicon compound having a molecular weight of 3,000 and having an epoxy group and having an epoxy equivalent of 0.5 mol/100 g at 25 ° C has the following molecular formula:
  • Fumed silica treated with dimethyldichlorosilane having an average particle diameter of 10 ⁇ m and a specific surface area of 300 m 2 /g
  • the semiconductor device LED lamp shown in FIG. 1 is packaged by providing a bracket 1 (100 W integrated bracket) to which the light-emitting element 2 is fixed, wherein the light-emitting element 2 (Sanan's S-23BBMUP-455 chip) passes through a bonding wire. 4 (Beijing Dabo Nonferrous Metal Solder Co., Ltd., specification 23um gold wire) is connected with the electrode 3, and the defoamed the above curable organopolysiloxane composition 5 of the present invention is coated and fixed by a dispenser. The holder 1 having the light-emitting element 2 is cured to obtain an integrated package.
  • the silicone polysiloxane mixture was poured into a mold, and heat-cured to form a film.
  • the baking conditions were: curing at 100 ° C for 1 hour and curing at 150 ° C for 3 hours.
  • the physical properties of the obtained film were measured, and the test results are shown in Table 1.
  • a sheet having a thickness of about 2 mm was prepared, kept at 100 ° C for 1 h, and then cured at 150 ° C for 3 h, and then the sheet was processed into a dumbbell shape and utilized at 25 ° C and 60% RH.
  • the universal material testing machine tests its tensile strength and elongation at break.
  • the viscosity was measured at 25 ° C using a rotational viscometer at 3 rpm and 12 rpm, and the thixotropic factor was a ratio of a viscosity of 3 rpm to a viscosity of 12 rpm.
  • composition After the obtained composition was defoamed, it was dispensed into a strip of 5 mm length, kept at 100 ° C for 1 h, and then cured at 150 ° C for 3 h. The height and width values were measured, and the height after curing was calculated. Width ratio.
  • test pass is indicated as ⁇ , and the test fails to be expressed as ⁇
  • Example 1-3 which contain the components (A1) (A2) (A2) of the present invention
  • the test results show that the thixotropic factors are all above 3.0, and have good thixotropy; Oil problem, good glass transmittance, 230 ° C 2h glass transmittance of more than 90%; In addition, it also has good heat resistance, all passed 260 ° C heat resistance 24h test.
  • Comparative Example 1 did not add (A3) component, which was not tested by heat resistance at 260 ° C for 24 h, and had a thixotropic factor of only 2.1, and the thixotropic property was poor, indicating that the (A3) component was an essential component.
  • composition of the present invention and the cured semiconductor device thereof not only have good heat resistance and oil-extracting properties, but also have good thixotropic properties.

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Abstract

L'invention concerne une composition d'organopolysiloxane thixotrope et un dispositif à semi-conducteur pour surmonter les défauts de l'art antérieur, la composition comprenant les composants suivants : (A1) un organopolysiloxane solide ayant une structure tridimensionnelle et comprenant un motif R1 3SiO1/2 et un motif SiO4/2 ; (A2) un organopolysiloxane liquide ayant une structure à chaîne linéaire et comprenant un motif R1 3SiO1/2 et un motif R2 2SiO2/2, les composants de (A2) ayant un poids moléculaire moyen en nombre inférieur à 10000 ; (A3) un organopolysiloxane liquide ayant une structure à chaîne linéaire et comprenant un motif R1 3SiO1/2 et un motif R2 2SiO2/2, les composants de (A3) ayant une masse moléculaire moyenne en nombre supérieure à 80 000 ; (B) un polyorganohydrogénosiloxane liquide ayant une structure à chaîne linéaire et comprenant un motif R3 3SiO1/2 et un motif R4 2SiO2/2; (C) un agent organosiloxane donnant du collant comprenant au moins un groupe époxy dans une molécule en moyenne ; (D) un agent thixotrope ; et (E) un catalyseur d'hydrosilylation à une dose pouvant favoriser le durcissement de la composition. Par comparaison à l'art antérieur, la composition et le dispositif à semi-conducteur durci à l'aide de celle-ci ont une bonne résistance à la chaleur et de bonnes propriétés de sortie de liquide, et présentent de bonnes performances thixotropes.
PCT/CN2015/072097 2014-12-03 2015-02-02 Composition d'organopolysiloxane thixotrope et dispositif à semi-conducteur WO2016086529A1 (fr)

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